CN115491784A - Preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity - Google Patents
Preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity Download PDFInfo
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- CN115491784A CN115491784A CN202211017697.4A CN202211017697A CN115491784A CN 115491784 A CN115491784 A CN 115491784A CN 202211017697 A CN202211017697 A CN 202211017697A CN 115491784 A CN115491784 A CN 115491784A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 104
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 104
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 102
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 98
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 47
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000000835 fiber Substances 0.000 title claims abstract description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 94
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 47
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000011165 3D composite Substances 0.000 claims abstract description 27
- -1 polypropylene Polymers 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 238000000866 electrolytic etching Methods 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 238000004070 electrodeposition Methods 0.000 claims description 7
- 229920000573 polyethylene Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000003068 static effect Effects 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 2
- 230000008018 melting Effects 0.000 abstract 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000000945 filler Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
Abstract
The invention relates to a preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity, which is characterized by comprising the following steps: (1) mixing an ethanol solution and a silane coupling agent to form a mixed solution; adding water into carbon fibers to prepare a suspension; mixing the mixed solution and the suspension, adding foamed nickel, performing ultrasonic treatment, centrifuging and drying to obtain a composite material; (2) Depositing a layer of graphene oxide on the surface of the composite material by taking the composite material as an anode, a platinum electrode as a cathode and the graphene oxide dispersion liquid as electrolyte to obtain a composite electrode; changing the electrolyte into a sodium chloride solution, carrying out electrolytic etching by taking the composite electrode as an anode to remove foamed nickel, and soaking in a hydrochloric acid solution to obtain a three-dimensional composite structure body; (3) Dispersing the three-dimensional composite structure in a dispersing agent, uniformly mixing with polypropylene, melting and blending to prepare a master batch, uniformly mixing the master batch with the polypropylene, melting and blending, and spinning. The invention has the advantages that: the process is simple, easy to control, safe and pollution-free, and the raw materials are easy to obtain; the product has excellent conductivity and can be used in the fields of static electricity and conductivity.
Description
Technical Field
The invention belongs to the technical field of composite materials, and relates to a preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity.
Background
With the rapid development of the plastic industry, polypropylene materials have been widely used in the fields of packaging, medical treatment, aerospace, machinery, electronics, construction, agriculture, and the like. The single polypropylene material can not meet the requirement of rapid development in the field of plastics, particularly has excellent insulating property, can be used in the field of insulating materials, but is easy to gather static charges to cause major accidents, and limits the application field of polypropylene.
The graphene is represented by sp 2 The graphene is a conductive nano material with a symmetrical hexagonal honeycomb lattice structure, the tensile strength of the graphene is as high as 130GPa, and the Young modulus is as high as 1TPa. The graphene is regarded as a semi-metal with zero band gap, the surface of the graphene has free electrons, the capability of conducting the electrons is strong, and the conductivity is 6000S/cm. Due to the excellent electrical and mechanical properties of graphene, the graphene becomes an ideal filler of insulating polymers, and mainly solves the problem of charge aggregation of the insulating polymers. However, the single graphene filler cannot meet the requirement of high-tech development, because the agglomeration phenomenon becomes more obvious after the concentration of the single graphene is increased, and the improvement space of the conductivity of the high polymer material is influenced.
The carbon fiber as one of carbon family members has the characteristics of low density, large length-diameter ratio, good flexibility, excellent conductivity and the like, and is one of excellent fillers for improving the conductivity and mechanical property of a high polymer material.
However, a composite material of polypropylene fiber, graphene and carbon fiber has not been disclosed.
Disclosure of Invention
The invention aims to make up for the defects of the existing material and provides a preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity. According to the invention, the graphene/carbon fiber three-dimensional composite structure is prepared, and then the graphene/carbon fiber/polypropylene fiber with excellent conductivity is prepared by a melt blending technology. The three-dimensional composite structure body is beneficial to the uniform dispersion of the filler in the high polymer material, the diffusion of charges and the improvement of the conductivity of the material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity is characterized by comprising the following steps:
(1) Preparation of carbon fiber/foamed nickel composite material
Mixing an ethanol aqueous solution with the mass concentration of 50-90% and a silane coupling agent according to the mass ratio of 100:2-5, mixing uniformly to form a mixed solution; adding carbon fibers into water, and ultrasonically stirring to prepare suspension with the concentration of 1-3 mol/L; mixing the mixed solution and the suspension according to a volume ratio of 1-1; centrifuging and drying (drying at 58-63 ℃ for 12-24 h) to obtain the carbon fiber/foamed nickel composite material;
(2) Preparation of graphene/carbon fiber three-dimensional composite structure
Depositing a layer of reduced graphene oxide on the surface of the carbon fiber/foamed nickel composite material by using an electrochemical deposition method by using carbon fiber/foamed nickel as an anode, a platinum electrode as a cathode and a graphene oxide dispersion liquid as an electrolyte to obtain a graphene/carbon fiber/foamed nickel composite electrode; changing the electrolyte into a sodium chloride solution, carrying out electrolytic etching by taking the graphene/carbon fiber/foamed nickel as an anode to remove the foamed nickel, and then soaking in a hydrochloric acid solution for 12 hours to obtain a graphene/carbon fiber three-dimensional composite structure;
(3) Preparation of graphene/carbon fiber/polypropylene fiber
According to the graphene/carbon fiber three-dimensional composite structure: dispersing the graphene/carbon fiber three-dimensional composite structure in a dispersing agent according to a mass ratio of 3: and (2) carrying out melt blending to prepare a master batch with the mass ratio of polypropylene being 1.
Further, in the step (1), the silane coupling agent is KH550, KH560, KH570 or KH792.
Further, the concentration of the graphene oxide dispersion liquid in the step (2) is 0.5-2mol/L.
Further, the concentration of the sodium chloride solution in the step (2) is 1.0-1.5mol/L.
Further, the concentration of the hydrochloric acid solution in the step (2) is 3.0-5.0mol/L.
Further, the dispersing agent in the step (3) is a mixture of N-methylpyrrolidone and polyethylene wax, wherein the weight ratio of N-methylpyrrolidone: the mass ratio of the polyethylene wax is 7.
Further, the device for melt blending in the step (3) is a twin-screw extruder, and the temperatures of the twin-screw extruder are respectively set to be 265 ℃,270 ℃,268 ℃ and 260 ℃.
Further, the spinning process conditions in the step (3) are as follows: the spinning temperature is 260-265 ℃, the air cooling temperature is 16-18 ℃, the humidity is 60-65%, and the spinning speed is 800-1000 m/min.
Further, the content of the graphene/carbon fiber three-dimensional composite structure in the graphene/carbon fiber/polypropylene fiber is 0.5% -3%.
According to the invention, foam nickel is used as a substrate, a layer of carbon fiber is coated by the foam nickel by using an impregnation technology to obtain a carbon fiber/foam nickel composite material, and a layer of reduced graphene oxide is deposited on the surface of the carbon fiber/foam nickel composite material by using an electrochemical deposition technology to obtain a graphene/carbon fiber/foam nickel composite electrode. And removing the foamed nickel by an electrolytic etching method to obtain the graphene/carbon fiber three-dimensional composite structure. And finally, preparing the graphene/carbon fiber/polypropylene fiber by a melt blending technology, wherein the preparation process is safe, simple and feasible, and the raw materials are easy to obtain. The graphene/carbon fiber/polypropylene fiber with excellent conductivity is obtained by manufacturing a master batch, adding a dispersing agent and constructing a graphene/carbon fiber three-dimensional composite structure so that the filler is uniformly dispersed in a polypropylene system. The falling-off of the filler can be prevented by a melt blending technology, and the graphene/carbon fiber/polypropylene fiber with more durable conductivity can be obtained. In addition, in the process of preparing the graphene/carbon fiber/foamed nickel composite material by electrochemical deposition, part of residual oxygen-containing functional groups of graphene can be used as a good dispersing agent for carbon fibers, and the graphene/carbon fiber three-dimensional composite structure keeps good dispersibility in a polypropylene system due to intercalation and isolation effects of the graphene and the carbon fibers.
The invention has the advantages that:
1. the invention has simple process, easy control, safety, no pollution and easy acquisition of raw materials;
2. when the mass fraction of the graphene/carbon fiber three-dimensional composite structure is 1% (the silane coupling agent is KH 550), the electrical conductivity of the graphene/carbon fiber/polypropylene fiber is 4.8 multiplied by 10 -7 S m -1 Conductivity 4.08X 10 compared to Polypropylene -13 S m -1 Improved by 6 orders of magnitude. After standing at room temperature for 10 days, the conductivity was 5.2X 10 -7 S m -1 After standing at room temperature for 20 days, the conductivity was 5.4X 10 -7 S m -1 After 30 days at room temperature, the conductivity was 5.4X 10 -7 S m -1 ；
3. The graphene/carbon fiber/polypropylene fiber prepared by the method disclosed by the invention is excellent in conductivity and can be applied to the fields of static electricity and conductivity.
Detailed Description
The present invention will be described in detail with reference to examples. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
A preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity comprises the following specific steps:
example 1
(1) Preparation of carbon fiber/foamed nickel composite material
Uniformly mixing 200mL of 60% ethanol aqueous solution with 4g of silane coupling agent KH560 to form a mixed solution; adding 3g of carbon fiber into 100mL of deionized water, and ultrasonically stirring for 1h to prepare a suspension; mixing the mixed solution and the suspension, adding 1.5mm multiplied by 2cm foamed nickel with porosity of 50-98% and pore diameter of 0.1mm-10mm, and carrying out ultrasonic treatment for 1h at 70 ℃; centrifuging and drying (drying at 60 ℃ for 12 hours) to obtain the carbon fiber/foamed nickel composite material;
(2) Preparation of graphene/carbon fiber three-dimensional composite structure
Taking carbon fiber/foamed nickel as an anode, a platinum electrode as a cathode, taking 1mol/L graphene oxide dispersion liquid as electrolyte, adjusting the pH of the solution to 11 by using 1mol/L NaOH, and depositing a layer of reduced graphene oxide on the surface of the carbon fiber/foamed nickel composite material by adopting an electrochemical deposition method to obtain a graphene/carbon fiber/foamed nickel composite electrode; changing the electrolyte into 1.0mol/L sodium chloride solution, carrying out electrolytic etching by taking graphene/carbon fiber/foamed nickel as an anode to remove foamed nickel, and then soaking in 5mol/L hydrochloric acid solution for 12 hours to obtain a graphene/carbon fiber three-dimensional composite structure;
(3) Preparation of graphene/carbon fiber/polypropylene fiber
Dispersing 120g of graphene/carbon fiber three-dimensional composite structure body in 40g of dispersing agent, wherein the dispersing agent is composed of N-methyl pyrrolidone and polyethylene wax according to a mass ratio of 7. And then uniformly mixing the master batch and polypropylene according to the mass ratio of 1.
In the graphene/carbon fiber/polypropylene fiber prepared in the embodiment 1 of the invention, the content of the graphene/carbon fiber is 1.00%; the moisture regain of the fiber is 12%, the moisture absorption and air permeability are good, and the electrical conductivity of the fiber reaches 5.0 multiplied by 10 -7 S/cm, tensile strength of 65.2MPa, bending strength of 78.4MPa, ammonia adsorption rate of 92.6%, and acetic acid adsorption rate of 90.3%.
Example 2
(1) Preparation of carbon fiber/foamed nickel composite material
Uniformly mixing 200mL of 70% ethanol water solution with mass concentration and 6g of silane coupling agent KH792 to form a mixed solution; adding 3g of carbon fiber into 100mL of deionized water, and ultrasonically stirring for 1h to prepare a suspension; mixing the mixed solution and the suspension, adding 1.5mm multiplied by 2cm foamed nickel with porosity of 50-98% and pore diameter of 0.1mm-10mm, and carrying out ultrasonic treatment for 1h at 70 ℃; centrifuging and drying (drying at 60 ℃ for 15 hours) to obtain the carbon fiber/foamed nickel composite material;
(2) Preparation of graphene/carbon fiber three-dimensional composite structure
Taking carbon fiber/foamed nickel as an anode, a platinum electrode as a cathode, taking 1.5mol/L graphene oxide dispersion liquid as electrolyte, adjusting the pH of the solution to 11 by using 1mol/L NaOH, and depositing a layer of reduced graphene oxide on the surface of the carbon fiber/foamed nickel composite material by adopting an electrochemical deposition method to obtain a graphene/carbon fiber/foamed nickel composite electrode; changing the electrolyte into 1.5mol/L sodium chloride solution, carrying out electrolytic etching by taking graphene/carbon fiber/foamed nickel as an anode to remove foamed nickel, and then soaking in 4mol/L hydrochloric acid solution for 12 hours to obtain a graphene/carbon fiber three-dimensional composite structure;
(3) Preparation of graphene/carbon fiber/polypropylene fiber
Dispersing 120g of a graphene/carbon fiber three-dimensional composite structure in 40g of a dispersing agent, wherein the dispersing agent is composed of N-methyl pyrrolidone and polyethylene wax according to a mass ratio of 7. And then uniformly mixing the master batch and polypropylene according to the mass ratio of 1.
According to the graphene/carbon fiber/polypropylene fiber prepared in the embodiment 2, the content of the graphene/carbon fiber is 1.25%; the moisture regain of the fiber is 13%, the moisture absorption and air permeability are good, and the electrical conductivity of the fiber reaches 4.3 multiplied by 10 -7 S/cm, tensile strength of 66.9MPa, bending strength of 80.6MPa, ammonia adsorption rate of 93.4%, acetic acid adsorption rate of 91.5%.
Example 3
(1) Preparation of carbon fiber/foamed nickel composite material
Uniformly mixing 200mL of 80% ethanol aqueous solution with 8g of silane coupling agent KH570 to form a mixed solution; adding 3g of carbon fiber into 100mL of deionized water, and ultrasonically stirring for 1h to prepare a suspension; mixing the mixed solution and the suspension, adding 1.5mm multiplied by 2cm foamed nickel with porosity of 50-98% and pore diameter of 0.1mm-10mm, and carrying out ultrasonic treatment for 1h at 70 ℃; centrifuging and drying (drying at 60 ℃ for 18 h) to obtain the carbon fiber/foamed nickel composite material;
(2) Preparation of graphene/carbon fiber three-dimensional composite structure
Taking carbon fiber/foamed nickel as an anode, a platinum electrode as a cathode, taking 2mol/L graphene oxide dispersion liquid as electrolyte, adjusting the pH of the solution to 11 by using 1mol/L NaOH, and depositing a layer of reduced graphene oxide on the surface of the carbon fiber/foamed nickel composite material by adopting an electrochemical deposition method to obtain a graphene/carbon fiber/foamed nickel composite electrode; changing the electrolyte into 1.5mol/L sodium chloride solution, carrying out electrolytic etching by taking graphene/carbon fiber/foamed nickel as an anode to remove foamed nickel, and then soaking in 3mol/L hydrochloric acid solution for 12 hours to obtain a graphene/carbon fiber three-dimensional composite structure;
(3) Preparation of graphene/carbon fiber/polypropylene fiber
Dispersing 120g of graphene/carbon fiber three-dimensional composite structure body in 40g of dispersing agent, wherein the dispersing agent is composed of N-methyl pyrrolidone and polyethylene wax according to a mass ratio of 7. And then uniformly mixing the master batch and polypropylene according to the mass ratio of 1.
Graphene/carbon fiber/polypropylene fiber and stone prepared in embodiment 3 of the invention1.43% graphene/carbon fiber content; the moisture regain of the fiber is 14%, the moisture absorption and air permeability are good, and the electrical conductivity of the fiber reaches 4.0 multiplied by 10 -7 S/cm, tensile strength of 67.3MPa, bending strength of 81.5MPa, ammonia adsorption rate of 93.9%, and acetic acid adsorption rate of 91.8%.
Finally, the following is explained: the contents mentioned in the invention are mass percentages except for special specifications. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of graphene/carbon fiber/polypropylene fiber with excellent conductivity is characterized by comprising the following steps:
(1) Preparation of carbon fiber/foamed nickel composite material
Mixing an ethanol aqueous solution with the mass concentration of 50-90% and a silane coupling agent according to the mass ratio of 100:2-5, mixing uniformly to form a mixed solution; adding carbon fibers into water, and ultrasonically stirring to prepare suspension with the concentration of 1-3 mol/L; mixing the mixed solution and the suspension according to a volume ratio of 1-1; centrifuging and drying to obtain the carbon fiber/foamed nickel composite material;
(2) Preparation of graphene/carbon fiber three-dimensional composite structure
Depositing a layer of reduced graphene oxide on the surface of the carbon fiber/foamed nickel composite material by using an electrochemical deposition method by using carbon fiber/foamed nickel as an anode, a platinum electrode as a cathode and a graphene oxide dispersion liquid as an electrolyte to obtain a graphene/carbon fiber/foamed nickel composite electrode; changing the electrolyte into a sodium chloride solution, carrying out electrolytic etching by taking the graphene/carbon fiber/foamed nickel as an anode to remove the foamed nickel, and then soaking in a hydrochloric acid solution for 12 hours to obtain a graphene/carbon fiber three-dimensional composite structure;
(3) Preparation of graphene/carbon fiber/polypropylene fiber
According to the graphene/carbon fiber three-dimensional composite structure: dispersing the graphene/carbon fiber three-dimensional composite structure in a dispersing agent according to a mass ratio of 3: and (2) carrying out melt blending to prepare a master batch with the mass ratio of polypropylene being 1.
2. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the silane coupling agent is KH550, KH560, KH570 or KH792.
3. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the drying condition in the step (1) is drying for 12-24h at 58-63 ℃.
4. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the concentration of the graphene oxide dispersion liquid in the step (2) is 0.5-2mol/L.
5. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the concentration of the sodium chloride solution in the step (2) is 1.0-1.5mol/L.
6. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the concentration of the hydrochloric acid solution in the step (2) is 3.0-5.0mol/L.
7. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the dispersing agent in the step (3) is a mixture of N-methylpyrrolidone and polyethylene wax, wherein the weight ratio of N-methylpyrrolidone: the mass ratio of the polyethylene wax is 7.
8. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the device for melt blending in the step (3) is a double-screw extruder, and the temperatures of the device are respectively set to be 265 ℃,270 ℃,268 ℃ and 260 ℃.
9. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the spinning process conditions in the step (3) are as follows: the spinning temperature is 260-265 ℃, the air cooling temperature is 16-18 ℃, the humidity is 60-65%, and the spinning speed is 800-1000 m/min.
10. The preparation method of the graphene/carbon fiber/polypropylene fiber with excellent conductivity as claimed in claim 1, wherein the preparation method comprises the following steps: the content of the graphene/carbon fiber/polypropylene fiber three-dimensional composite structure body is 0.5% -3%.
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Citations (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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